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Role of assisting reagents on the synthesis of α-Fe2O3 by microwave-assisted hydrothermal reaction

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Abstract

Currently, the controlled synthesis of well-defined metal oxide nanoparticles has received intense scientific attention to modulate the properties of materials through the size and shape. This paper focuses on providing a better understanding about the growth, morphology, size, and crystal structure of α-Fe2O3 nanoparticles synthesized by a microwave-assisted hydrothermal route, considering a detailed analysis of the influence of the reaction temperature, time, and ratio of assisting reagents (sodium citrate and urea) as well as the effects of calcination temperature. According to X-Ray Diffraction analysis, the α-Fe2O3 crystalline phase was directly prepared at 200 °C for 60 min using only urea, while materials with low crystallinity were obtained using only sodium citrate as well as sodium citrate:urea (in both ratio 1:1 and 2:2.5). Upon calcination at 600 °C, the crystallization of α-Fe2O3 started in the material prepared with a sodium citrate:urea ratio of 2:2.5. Scanning and Transmission Electron Microscopies results revealed that the materials synthesized using urea, sodium citrate, and sodium citrate:urea ratio of 1:1 are formed by nanoparticles less than 100 nm without a defined morphology, whereas the materials prepared using sodium citrate:urea ratio of 2:2.5 showed well-defined nanospheres with average sizes between 150 and 250 nm constituted by self-assembled crystals smaller than 10 nm. The shape and size of the nanospheres did not undergo significant changes even at high thermal treatments, such as 800 °C. Based on equilibrium diagrams, the role of each chemical agent was disclosed, indicating that the modulated precipitation through soluble complexes is a very important factor in controlling the hierarchical organization of the particles to form the nanospheres. This study demonstrates the versatility of sodium citrate and urea as assisting reagents to prepare a variety of α-Fe2O3 nanoparticles. Besides, these results could be useful in extending new ideas for the synthesis of other nanomaterials.

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Acknowledgements

The authors thank Consejo Nacional de Ciencia y Tecnología from Mexico (CONACYT) for funding, to LANNBIO Cinvestav-Mérida for the use of the facilities, as well as the technical assistance of Daniel Aguilar and Dora Huerta.

Funding

This research was funded by Consejo Nacional de Ciencia y Tecnología from Mexico (CONACYT) through the projects: Cátedra 1710, INFR-2015-01-252758 and CB-2015-255109 as well as the support to LANNBIO Cinvestav-Mérida by the Grants FOMIX Yucatán 2008-108160, CONACYT LAB-2009-01-123913, 188345, 204822, 292692 and 294643.

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  1. CONACYT-Departamento de Física Aplicada, CINVESTAV-IPN, Antigua Carretera a Progreso km 6, 97310, Mérida, Yucatán, Mexico

    Miguel A. Ruiz-Gómez

  2. Departamento de Física Aplicada, CINVESTAV-IPN, Antigua Carretera a Progreso km 6, 97310, Mérida, Yucatán, Mexico

    Miguel A. Ruiz-Gómez & Geonel Rodríguez-Gattorno

  3. Facultad de Ingeniería Civil, Universidad Autónoma de Nuevo León, UANL, 66455, San Nicolás de los Garza, Nuevo León, Mexico

    Mayra Z. Figueroa-Torres

  4. CICFIM-Facultad de Ciencias Físico Matemáticas, Universidad Autónoma de Nuevo León, UANL, Av. Universidad S/N, San Nicolás de los Garza, 66455, Nuevo León, Mexico

    Sergio Obregón

  5. Instituto de Física, UNAM, Circuito de la Investigación s/n, Ciudad Universitaria, Coyoacán, 04510, Mexico City, Mexico

    Samuel Tehuacanero-Cuapa & Manuel Aguilar-Franco

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MAR-G contributed to synthesis, caracterization, discussion, and writing. GR-G, MZF-T, and SO performed discussion and writing. ST-C was involved in characterization, discussion, and writing. MA-F contributed to characterization and discussion. All the authors have approved the final version of this manuscript.

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Correspondence to Miguel A. Ruiz-Gómez.

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Ruiz-Gómez, M.A., Rodríguez-Gattorno, G., Figueroa-Torres, M.Z. et al. Role of assisting reagents on the synthesis of α-Fe2O3 by microwave-assisted hydrothermal reaction. J Mater Sci: Mater Electron 32, 9551–9566 (2021). https://doi.org/10.1007/s10854-021-05618-x

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